Determination of antimony and the differential determination of antimony(III) and antimony(V) by ICP-AES and high-resolution ICP-MS with a hydride generation technique

Abstract

Simple methods for the chemical speciation of antimony and organotin compounds were developed by atomic spectroscopy. Antimony was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) and high-resolution inductively coupled plasma mass spectrometry (ICP-MS) with a hydride generation technique. Stibine generated with sodium tetrahydroborate(III) (SBH) in a mixing coil was separated from solution with a spiral tube in a closed vessel. The antimony contents of River Arakawa were determined by the present methods. Antimony(III) and antimony(V) were determined differentially by ICP-AES and ICP-MS. Antimony(III) was determined at pH 5.5, while the total antimony was determined at pH 1.0 using potassium iodide as a prereductant. It was found by ICP-MS that the antimony(III) contents of River Arakawa increased while the antimony(V) contents decreased while descending down-stream. Tributyltin and triphenyltin in fish were determined by gas chromatography-atomic absorption spectrometry (GC-AAS) with hydride generation. Fish meat was homogenized in a hydrochloric acid solution of 8-quinolinol. The chlorides in fish were extracted into hexane. After the solvent had been converted to 2-propanol, the solution was applied to a Bondesil SCX solid sorbent. The organotin compounds were eluted with a methanol solution of hydrochloric acid and determined by GC-AAS after hydradization with SBH. The organotin chlorides are supposed to form ion-associates with 8-hydroquinolinium cation in a hydrochlic acid medium.